Ageing of bread has ge n e rated re s e a rch interest fo r m a ny ye a rs. It is a phenomenon involving starch which is a polysaccharide made up of two components, amylose and amylopectin. Both are polymers of glucose but amylose is linear while amylopectin has a branched structure. In the starch granule, the amylose and amylopectin are intermingled but when the linear segments of a mylopectin align they become ord e red into cry s t a l l i t e s . During the baking of bread, an order to disorder transition occurs in which the starch granules present in the flour swell and some of the amylose diffuses out of the granule destroying the crystalline structure. This process is essentially reversed during the ageing of bread as crystallinity slowly redevelops in the amylopectin fraction [1]. This crystallinity is responsible for the increase in firmness in the bread Differential scanning calorimetry and near infrared (NIR) reflectance spectroscopy have been used to follow the development of crystallinity in stored bread. Using each technique, changes in measured properties were apparent which, when fitted by first-order exponential equations, gave calculated rate constants of similar magnitude. It is postulated that each technique is giving complementary information about the changes taking place in the amylopectin fraction of the bread crumb.